反应详情

温度

0 °C

A solution of 1-(1,4-dioxa-spiro[4.5]dec-8-yl)-4-(4-fluoro-phenyl)-piperazine (3.13 gm) (C18H25FN2O2) in 100 ml 3N hydrochloric acid and 100 ml dioxane was stirred at ambient temperature for 2 hours. The mixture is cooled to 0° C., neutralized with 2N sodium hydroxide and extracted with 2×100 ml ethyl acetate. The ethyl acetate layer was washed with water and brine (each 2×40 ml), dried over sodium sulfate and concentrated to a solid. This material, which was recrystallized from ethyl ether (1.5 gm), has a melting point of 104-106° C.

1. extractionextracted with 2×100 ml ethyl acetate
2. washThe ethyl acetate layer was washed with water and brine (each 2×40 ml),
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated to a solid
5. customThis material, which was recrystallized from ethyl ether (1.5 gm)